Triphenylphosphine → HCID 87426500, compound

Participants

Reaction Steps

To a stirred solution of methyl 4-hydroxy-3-methylbenzoate (1.5 g, 9.0 mmol), 2,2-difluoroethanol (0.90 g, 10.8 mmol), triphenylphosphine (3.6 g, 13.5 mmol) in THF (40 mL) is added dropwise diethyl azodicarboxylate (4.9 mL, 10.8 mmol, 40% solution in toluene) at 0° C. The mixture is stirred at room temperature for 30 minutes, and then at 60° C. for 2 hours. After cooled to room temperature, the mixture is concentrated under reduced pressure. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (18:1) to give 1.9 g (90% yield) of the title compound as a white solid.

Provenance & Evidence